EP2892986B1 - Procédé de traitement d'une composition de graisse végétale - Google Patents

Procédé de traitement d'une composition de graisse végétale Download PDF

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Publication number
EP2892986B1
EP2892986B1 EP12772211.4A EP12772211A EP2892986B1 EP 2892986 B1 EP2892986 B1 EP 2892986B1 EP 12772211 A EP12772211 A EP 12772211A EP 2892986 B1 EP2892986 B1 EP 2892986B1
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EP
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Prior art keywords
vegetable fat
fat composition
fraction
free fatty
fatty acids
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EP12772211.4A
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German (de)
English (en)
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EP2892986A1 (fr
Inventor
Rasmus Leth MILLER
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AAK AB
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AAK AB
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/06—Refining fats or fatty oils by chemical reaction with bases
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/003—Refining fats or fatty oils by enzymes or microorganisms, living or dead
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/04—Refining fats or fatty oils by chemical reaction with acids
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
    • C11C3/08—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with fatty acids

Definitions

  • the invention relates to a process according to claim 1.
  • the invention relates to a method for processing a vegetable fat composition.
  • Several problems may exist in relation to such processing being expensive and difficult. Therefore, it is an object of the invention to provide a method for processing a vegetable fat in a cost-effective and efficient way.
  • the invention relates to a method for processing a vegetable fat composition, the method comprising the steps of
  • a said first fraction being rich in StOO and/or OOO is meant that StOO and/OOO comprises a significant part of the first fraction.
  • a first fraction may comprise StOO and/or OOO in amount exceeding the content of any other components or types of triglycerides.
  • such a first fraction may comprise more than 40 % by weight of StOO and/or OOO, such as more than 50 % by weight of StOO and/or OOO, such as more than 60 % by weight of StOO and/or OOO.
  • StOO may be dominating, due to the fact that StOO typically will be the lower melting point triglyceride with the highest concentration.
  • a second fraction being rich in StOSt it may for example comprise StOSt in amount exceeding the content of any other components or types of triglycerides. Also, such a second fraction may comprise more than 40 % by weight of StOSt, such as more than 50 % by weight of StOSt, such as more than 60 % by weight of StOSt, such as more than 70% by weight of StOSt.
  • the separation step is meant a process for separating the neutralized vegetable fat composition into the first and second fractions.
  • This separation step may preferably be a fractionation.
  • fractionation is a fractional crystallization, which is to be understood as a separation process in which one fraction is separated from another fraction by crystallization.
  • Such fractional crystallization is preferably performed by heating the neutralized vegetable fat composition, preferably until it is completely melted, and then cooling the neutralized vegetable fat composition until the second fraction crystallizes and can be removed from the second fraction, which is a liquid remaining or left-over fraction.
  • the fractional crystallization preferably involves a solvent, such as adding a solvent before the cooling of the neutralized vegetable fat composition, and preferably before the step of heating the neutralized vegetable fat composition. Also, this solvent is preferably removed from the first and/or second fraction after the separation for the two fractions.
  • the solvent may preferably be hexane or acetone.
  • the separation step may be a distillation step or involve other separation steps, or be a combination of several separation steps.
  • the separation step may be more efficient, especially when this involves a fractionation step.
  • the fractionation step is more effective when said first neutralization step may be performed, since no or at least very little of free fatty acids are present to disturb the crystallization processes that are essential to the fractionation. Since the fractionation step relies largely on crystallization, it is imperative that the crystallization characteristics of a fat to be fractionated are suitable for fractionation, as opposed to some fats, where a large content of free fatty acids may change the crystallization characteristics and impair the fractionation. However, after performing said first neutralization such free fatty acids are not present in the neutralized vegetable fat composition, at least not at significant levels.
  • residues of acids may be removed or reacted, thereby significantly increasing the lifetime of the enzymes.
  • residues of acids may include acids from storage, bi-products from the fractionation process and/or acids added in the first neutralization step.
  • the first neutralization step comprises a base adding step or a distilling step it may be advantageous to add an acid before and/or after the base adding step or the distilling step. Therefore, in such embodiments, it is a particular advantage to add the second base, since residues of these acids may then be neutralized.
  • a lesser amount of neutralized vegetable fat composition has to be neutralized by adding the second base.
  • the neutralized vegetable fat composition may be fractionated approximately 1:1 into a first and a second fraction.
  • the fat has to be neutralized in the second neutralization step. This may be advantageous in both that a smaller amount of second base has to be added, and in that the process equipment only has to handle about half the amount of fat.
  • the time between the second neutralization step and the transesterification step may be reduced, thereby diminishing the build-up of substances that may be harmful to the enzymes; such build-up may otherwise take place over time.
  • by-products from the fractionation may be handled by or in relation to the second neutralization step, thereby providing a better product.
  • the present invention provides a method for preparing a vegetable fat composition for fractionation, while preparing the lower melting point first fraction from the fractionation to subsequently be subjected to an enzymatic transesterification.
  • the lower melting point first fraction which is a low value part or fraction of the vegetable fat composition, may be enzymatically upgraded, thus increasing the value of this part or fraction significantly.
  • said first neutralization step comprises the steps of
  • fatty acids in the vegetable fat composition are saponified, i.e. the fatty acids are converted or transformed into saponified fatty acids, i.e. soaps. It is to be understood that fatty acids refer to free fatty acids, and therefore not fatty acids that form part of e.g. triglycerides.
  • the free fatty acids in the vegetable fat composition may have characteristics, which are substantially different from those of the main substances of the vegetable fat composition, namely the triglycerides, it is advantageous to remove these free fatty acids from the vegetable fat composition.
  • the base adding step does not remove the free fatty acids, but rather converts them into soaps, it facilitates the subsequent step of removing the free fatty acids in the form of soaps in the soap separation step.
  • any residues of saponified free fatty acids into free fatty acids may result in a reduced fractionation capacity, e.g. by partial clogging of fractionation filters or other equipment. Therefore, by adding the first acid, such potential fractionation capacity reduction is eliminated.
  • the saponified free fatty acids may then aggregate on equipment and block narrow passages, such as e.g. filters in the fractionation process, which is highly disadvantageous. This may be a problem even for relatively small amounts of saponified free fatty acids left in the vegetable fat composition by the separation process.
  • This problem is solved, however, by converting the saponified free fatty acids back into free fatty acids by adding the first acid. Thereby, passage blocking by aggregated saponified free fatty acids is avoided, while the relatively small amount of free fatty acids may be insufficient to disturb the fractionation process.
  • said first neutralization step comprises a distillation step of distilling free fatty acids from the vegetable fat composition thereby obtaining a neutralized vegetable fat composition.
  • An advantage of the above embodiment is that by removing the free fatty acids or at least the larger part thereof from the vegetable fat composition, the separation efficiency of the subsequent separation may be significantly increased, especially when using fractionation in the separation step.
  • said first neutralization step furthermore comprises adding a first acid to the vegetable fat composition before the distilling step.
  • the vegetable fat composition By adding the first acid before the distilling step, the vegetable fat composition has a decreased tendency to discolor during the distilling step. This effect is especially pronounced when a step of bleaching the vegetable fat composition is performed after the addition of the first base, and before the distilling step.
  • said first neutralization step furthermore comprises adding a first acid to the vegetable fat composition or a product.
  • this could e.g. be a pre-treatment step, such as right before e.g. a distilling step, or as a post-treatment step, such as after e.g. adding the first base adding step.
  • Adding the first acid may increase the yield and/or quality of the neutralized vegetable fat.
  • said first acid is phosphoric acid.
  • the first acid may e.g. be citric acid.
  • said first neutralization step furthermore comprises bleaching said vegetable fat composition before said distilling step.
  • the vegetable fat composition has a decreased tendency to discolor during the distilling step. This bleaching is preferably performed after step of adding a first base to the vegetable fat composition.
  • the vegetable fat composition comprises shea fat.
  • an advantage of the above embodiment is that the process for treatment of the vegetable fat composition according to the invention is particularly suitable for treatment of fats with a high content of free fatty acids, hereunder especially shea fat extracted from shea nuts, and also known as shea oil or shea butter.
  • shea fat extracted from shea nuts
  • shea oil or shea butter Only a part of a shea fat being the first fraction being the higher melting point fraction, which may for instance constitute about e.g. half of the shea fat, can be used e.g. as a component in cocoa butter equivalent (CBE).
  • CBE cocoa butter equivalent
  • the part of the shea fat to be transesterified must be processed in order to be enzyme compatible, i.e. to facilitate a satisfactory lifetime of the enzyme, and hence permit a cost-effective process of treatment of the shea fat.
  • the process of the present embodiment solves these and other problems and increases the StOSt rich part of a shea fat for use in e.g. a CBE.
  • the problems of fractionating a vegetable fat composition comprising free fatty acids and/or soap residues thereof, and the problem of short enzyme lifetime are solved by the invention.
  • shea fat has an extraordinary large content of free fatty acids, whereas other fats may have a lower content of free fatty acids, the above mentioned problems and/or other problems associated with free fatty acids may be especially pronounced for shea fat, and therefore the solution to these problems is particularly advantageous for application of the treatment process according to the invention on shea fat.
  • the vegetable fat composition comprises refined shea fat.
  • the neutralized first fraction is bleached.
  • the bleaching may be performed by adding bleaching earth to the neutralized first fraction.
  • the step of bleaching is performed after the second neutralization step, and before the enzymatic transesterification step.
  • the bleaching step preferably comprises filtering of the bleaching earth from the neutralized first fraction.
  • Such saponified free fatty acids may otherwise have a negative effect on the crystallization characteristics of the first fraction, thereby potentially decreasing the efficiency of subsequent fractionations, such as fractionations after the transesterification, and furthermore such saponified free fatty acids may induce a very bad taste in the first fraction or products comprising part of the first fraction, such as chocolate-products comprising cocoa butter equivalent based on the first fraction and a palm oil mid fraction.
  • saponified free fatty acids may induce such bad taste in the fat and/or products thereof.
  • a further advantage of the bleaching step is that metal residues in the first fraction, such as metal residues from the fractionation equipment, may be removed in the bleaching step.
  • a palm oil mid fraction may be understood as different palm oil products.
  • the PMF should be understood as a hard PMF having an iodine value of 30 to 35, such as 32, 33, or 34.
  • a softer PMF having a higher iodine value of up to e.g. 50 may be usable.
  • the separation step involves a fractionation step.
  • the fractionation step is a separation process in which one fraction is separated from another fraction by crystallization, i.e. a fractional crystallization.
  • Such fractional crystallization is preferably performed by heating the neutralized vegetable fat composition, preferably until it is completely melted, and then cooling the neutralized vegetable fat composition until the second fraction crystallizes and can be removed from the first fraction, which is a liquid remaining or left-over fraction.
  • cooling the neutralized vegetable fat composition is to be understood a process, in which the neutralized vegetable fat composition has a lower temperature after the cooling compared to before the cooling, and the cooling may therefore involve keeping the temperature constant or even raising the temperature.
  • the cooling step may involve multiple cooling and heating steps, and steps of keeping the temperature constant.
  • the fractional crystallization preferably involves a solvent, such as adding a solvent before the cooling of the neutralized vegetable fat composition, and preferably before the step of heating the neutralized vegetable fat composition. Also, this solvent is preferably removed from the first and/or second fraction after the separation for the two fractions.
  • the solvent may preferably be hexane or acetone.
  • the first base comprises an aqueous solution of NaOH.
  • the first base may comprise NaOH (sodium hydroxide) in another form, such as in crystalline form, or the second base may comprise other suitable bases in suitable forms, such as aqueous solutions.
  • suitable bases may preferably be foodstuff-compatible strong bases, and may include KOH (potassium hydroxide), or lithium hydroxide (LiOH), or lithium carbonate (Li2CO3), or calcium hydroxide (Ca(OH)2), or barium hydroxide (Ba(OH)2), sodium carbonate (Na2CO3), sodium bicarbonate (NaHCO3), or other suitable bases.
  • the first base comprises a 50% w/w aqueous solution of NaOH.
  • the concentration of the first base may be between 5 and 90% w/w, such as between 10 and 70% w/w, such as between 15 and 65% w/w, such as between 15 and 60 % w/w, such as between 15 and 55% w/w, for example the concentration of the first base may preferable be 20 % w/w.
  • the amount of the first base added to the vegetable fat composition in the base adding step is based on the amount of free fatty acids in the vegetable fat composition.
  • the amount of the first base added to the vegetable fat composition is adapted to the amount of free fatty acids in the vegetable fat composition.
  • said amount of first base being based on said amount of free fatty acids may be meant that the amount of first base is calculated from the amount of the free fatty acids.
  • the amount of free fatty acids is in this context to be understood as e.g. an estimated value, i.e.
  • This may e.g. be done by measuring the amounts of free fatty acids in the vegetable fat composition and adapting the amount of the first base based on such measurements.
  • a measurement of the amount of free fatty acids may e.g. be a measurement of the pH-value in the vegetable fat composition and/or in the base added vegetable fat composition.
  • the amount of the first base added to the vegetable fat composition in the base adding step is based on the acidity of the vegetable fat composition.
  • the amount of the first base added to the vegetable fat composition is adapted to the amount of acidity of the vegetable fat composition.
  • said amount of first base being based on said amount of free fatty acids may be meant that the amount of first base is calculated from the amount of the free fatty acids.
  • the amount of free fatty acids is in this context to be understood as e.g. an estimated value, i.e.
  • the molar amount of the first base added to the vegetable fat composition in the base adding step is between 0.5 and 3 times the molar amount of the free fatty acids in the vegetable fat composition, such as between 0.8 and 2 times the molar amount of the free fatty acids in the vegetable fat composition, such as between 1 and 2 times the molar amount of the free fatty acids in the vegetable fat composition, such as between 1.2 and 1.4 times the molar amount of the free fatty acids in the vegetable fat composition, such as 1.3 times the molar amount of the free fatty acids in the vegetable fat composition.
  • the amount of the first base added in the base adding step may be calculated from the percentage of free fatty acids in the vegetable fat composition. This percentage of free fatty acids may be estimated or calculated, or a combination of measured data and estimations. Furthermore, measurements may also include e.g. measurements of a pH-value in the vegetable fat composition, e.g. by measuring a pH-value in a water phase extracted from the vegetable fat composition.
  • the amount of the first base added to the vegetable fat composition in the first neutralization step is found by measuring and/or estimating the concentration in percent by weight of free fatty acids in the vegetable fat composition as a first free fatty acid concentration; then calculating a second free fatty acid concentration as by adding between 0.3 and 0.9, such as 0.6, to the numeric value of the first free fatty acid concentration; then calculating an amount of the first base equivalent to the calculated second free fatty acid concentration.
  • the concentration of other acids may be incorporated, so that the concentration of acids replaces the concentration of free fatty acids.
  • the first free fatty acid concentration may e.g. be measured and/or estimated to be 9.5 percent by weight.
  • the second free fatty acid concentration may be calculated by adding e.g. 0.6 according to the above to the numeric value of the first free fatty acid concentration, i.e. adding 0.6 to 9.5, thereby obtaining a second free fatty acid concentration of 10.1 percent. From this the amount of equivalent first base may be calculated.
  • the amount of the first base that is added to the vegetable fat composition in the base adding step is to between 1 g and 500 g, such as between 5 g and 50 g, such as between 11 g and 22 g for each kilogram of the vegetable fat composition, such as between 14.7 g and 18.4 g.
  • the above mentioned amounts of the first base may e.g. be added as a 50 % w/w aqueous solution of e.g. NaOH. Then, the above amounts correspond to between 2 g and 1000 g, such as between 10 g and 100 g, such as between 22 g and 44 g for each kilogram of the vegetable fat composition, such as between 27 g and 39 g for each kilogram of the vegetable fat composition, such as between 29.4 g and 36.8 g. It should be noted, however, that for different batches of vegetable fat compositions, the amount of free fatty acids may vary. Therefore, the amount of first base added to the vegetable fat composition may vary accordingly, and the above mentioned amounts of the first base may cover various concentrations of free fatty acids according to the above embodiment.
  • the second base comprises an aqueous solution of NaOH.
  • the second base may comprise NaOH (sodium hydroxide) in another form, such as in crystalline form, or the second base may comprise other suitable bases in suitable forms, such as aqueous solutions.
  • suitable bases may preferably be foodstuff-compatible strong bases, and may include KOH (potassium hydroxide), or lithium hydroxide (LiOH), or lithium carbonate (Li2CO3), or calcium hydroxide (Ca(OH)2), or barium hydroxide (Ba(OH)2), sodium carbonate (Na2CO3), sodium bicarbonate (NaHCO3), or other suitable bases.
  • the second base comprises a 50% w/w aqueous solution of NaOH.
  • the concentration of the second base may be between 5 and 90% w/w, such as between 10 and 70% w/w, such as between 15 and 65% w/w, such as between 15 and 60 % w/w, such as between 15 and 55% w/w, preferably between 20 and 50 % w/w.
  • the molar amount of the second base added to the first fraction in the second neutralization step is between 0.5 and 3 times the molar amount of the free fatty acids in the first fraction, such as between 0.8 and 2 times the molar amount of the free fatty acids in the first fraction, such as between 1 and 2 times the molar amount of the free fatty acids in the first fraction, such as between 1.2 and 1.4 times the molar amount of the free fatty acids in the first fraction, such as 1.3 times the molar amount of the free fatty acids in the first fraction.
  • the amount of the second base added to the first fraction in the second neutralization step is found by measuring and/or estimating the concentration in percent by weight of free fatty acids in the first fraction as a first free fatty acid concentration; then calculating a second free fatty acid concentration as by adding between 0.3 and 0.9, such as 0.6, to the numeric value of the first free fatty acid concentration; then calculating an amount of the second base equivalent to the calculated second free fatty acid concentration.
  • the concentration of other acids may be incorporated, so that the concentration of acids replaces the concentration of free fatty acids.
  • the first free fatty acid concentration may e.g. be measured and/or estimated to be 9.5 percent by weight.
  • the second free fatty acid concentration may be calculated by adding e.g. 0.6 according to the above to the numeric value of the first free fatty acid concentration, i.e. adding 0.6 to 9.5, thereby obtaining a second free fatty acid concentration of 10.1 percent. From this the amount of equivalent second base may be calculated.
  • the amount of the second base added to the first fraction may be calculated from the percentage of free fatty acids in the first fraction.
  • the amount of the second base that is added to the first fraction in the second neutralization step is between 0.1 and 2 for each kilogram of vegetable fat composition provided, such as between 0.45 g and 0.9 g, such as between 0.6 g and 0.75 g.
  • the above mentioned amounts of the second base may e.g. be added as a 50 % w/w aqueous solution of e.g. NaOH. Then, the above amounts correspond to between 0.2 and 4 for each kilogram of vegetable fat composition provided, such as between 0.9 g and 1.8 g, such as between 1.2 g and 1.5 g.
  • the soap separation step comprises
  • the soap separation step comprises
  • the base added vegetable fat composition is washed twice, or several times. Again, advantage is taken of the fact that the saponified free fatty acids has an increased solubility in water and decreased solubility in the base added vegetable fat composition compared to the free fatty acids.
  • the washing is preferably performed once or several times after the centrifuging of the base added vegetable fat composition, i.e. the washing is subsequent to the centrifugation.
  • soap separation step comprises
  • drying of the base added vegetable fat composition is according to one embodiment meant that the water content is lowered. According to one embodiment the drying of the base added vegetable fat composition is performed after washing the base added vegetable fat composition.
  • the base added vegetable fat composition is adapted by the process steps to be transesterified by transesterification enzymes, while maintaining a satisfactory and economically cost-effective lifetime of the enzymes, while at the same time minimizing the production of diglycerides, thereby avoiding to render the valuable transesterified vegetable fat composition less valuable.
  • the shelf lifetime of this base added vegetable fat composition, the second fraction, the transesterified first fraction, and/or any other fractions or products thereof may be extended. This could e.g. be due to prevention or inhibition of hydrolysis due to low water content. Even further, efficiency of bleaching steps of such fats is increased significantly, e.g. due to prevention of the bleaching earth agglomerating due to water content.
  • the drying is performed subsequent to the washing of the base added vegetable fat composition, which is preferably performed after the centrifugation of the base added vegetable fat composition.
  • the first acid comprises citric acid.
  • the first acid is a citric acid, in the form of e.g. an aqueous solution or in solid or crystalline form.
  • the first acid may include other acids, such as isocitric acid, aconitic acid, and propane-1,2,3-tricarboxylic acid (tricarballylic acid, carballylic acid), or another weak organic acid, such as oxalic acid or acetic acid, or other weak acids.
  • the first acid comprises an aqueous solution of citric acid in a concentration of between 1 and 90 % w/w, such as between 5 and 80 % w/w, such as between 10 and 60 % w/w, such as between 15 and 40 % w/w, such as between 15 and 30 % w/w, such as between 18 and 25 % w/w, such as 20 % w/w.
  • the amount of the first acid that is added to the first fraction is between 10 g and 200 g per 1000 kilogram of the first fraction, such as between 20 g and 100 g, such as between 67 g and 60 g, such as 65 g.
  • This may e.g. be added as a 20 % w/w aqueous solution of an acid, such as e.g. citric acid.
  • the above amounts then correspond to between 50 g and 1000 g per 1000 kilogram of the first fraction, such as between 100 g and 500 g, such as between 200 g and 300 g, such as 250 g.
  • the amount of the first acid may also be larger or smaller. It should be noted that adding an excess amount of the first base may only result in material waste of the first base, i.e. the amount of the first base may in some embodiments not need specific adjustment when exceeding a threshold value corresponding to a satisfactory conversion of saponified free fatty acids into free fatty acids.
  • the first acid transforms any residual saponified free fatty acids in the reduced vegetable fat composition into free fatty acids.
  • an advantage of the above embodiment is that the fractionation step may be performed in an optimized way without clogging of fractionation filters, which may lead to lower fractionation capacity or to halting the fractionation completely to exchange or clean such soap residue clogged filters. Therefore, it is an advantage to transform or convert residual saponified free fatty acids, i.e. small amounts of saponified free fatty acids, into free fatty acids.
  • residual or small amounts of saponified free fatty acids is meant low concentrations e.g. in relation to the total volume, or to the initial amount of free fatty acids, i.e. the amount of free fatty acids before the soap separation step, such as in the base added vegetable fat composition.
  • residues of citric acid are removed by adding the second base.
  • An advantage of the above embodiment is that the lifetime of the enzymes is increased by removing the citric acid which is left-over after the conversion or transformation of the residues of saponified free fatty acids into free fatty acids. Thereby, it is facilitated that the fractionation can be performed effectively without filter clogging, while at the same time having a sufficiently long lifetime of the enzymes.
  • removing an acid may in an embodiment be meant transforming or converting the acid into a non-acid, such as a salt.
  • the concentration of citric acid in the neutralized first fraction is lower than 10 ppm by weight, such as lower than 5 ppm by weight, such as lower than 2 ppm by weight, such as lower than 1 ppm by weight, such as lower than 0.75 ppm by weight, such as lower than 0.5 ppm by weight, such as lower than 0.3 ppm by weight, such as lower than 0.2 ppm by weight, such as lower than 0.1 ppm by weight, such as lower than 0.05 ppm by weight, such as lower than 0.3 ppm by weight, such as lower than 0.2 ppm by weight, such as lower than 0.01 ppm by weight, after adding the second base.
  • concentrations of citric acid is to be understood concentrations of citric acid or dissolved citric acid, i.e. as opposed to a citric acid in the form of a salt.
  • the concentration of acids in the neutralized first fraction is lower than 10 mmol/100g of the first fraction, such as lower than 5 mmol/100g of the first fraction, such as lower than 2 mmol/100g of the first fraction, such as lower than 1 mmol/100g of the first fraction, such as lower than 0.75 mmol/100g of the first fraction, such as lower than 0.5 mmol/100g of the first fraction, such as lower than 0.3 mmol/100g of the first fraction, such as lower than 0.2 mmol/100g of the first fraction, such as lower than 0.1 mmol/100g of the first fraction, such as lower than 0.05 mmol/100g of the first fraction, such as lower than 0.3 mmol/100g of the first fraction, such as lower than 0.2 mmol/100g of the first fraction, such as lower than 0.01 mmol/100g of the first fraction, after second neutralization.
  • concentrations of acids is to be understood concentrations of acids or dissolved acids, i.e. as opposed to acids in the form of salts. Therefore, the above mentioned concentrations may well be understood in relation to a pH-value in the neutralized first fraction, or in a water phase extracted from the neutralized first fraction.
  • the neutralized first fraction is completely neutralized.
  • a neutralized first fraction may in one embodiment be meant that if a water ph-ase is extracted from the vegetable fat of the neutralized first fraction, said water phase is neutralized, e.g. with respect to pH-value or with respect to the concentration of free fatty acids.
  • an excess amount of first base may be added such that the term completely neutralized should be understood as the extracted water phase having a neutral or basic pH-value or that the saponification of the free fatty acids is complete or at least substantially complete, such as at least 80 % w/w, such as at least 90 % w/w, such as at least 95 % w/w, such as at least 98% w/w, such as at least 99 % w/w.
  • excess amounts of the first base may result in a loss of fat from the neutralized first fraction, and therefore such excess amounts of first base should, if possible, be minimized.
  • the enzymes with transesterification activity are 1,3-specific enzymes.
  • the enzymes are lipase, such as a 1,3-specific lipase.
  • 1,3-specific lipases may e.g. be lipases of Rhizopus delemar, Mucor miehei, Aspergillus niger, Rhizopus arrhizus, Rhizopus niveus, Mucor javanicus, Rhizopus javanicus, Rhicomucor miezei, and Rhizopus oxyzae.
  • Other 1,3-specific lipases may also be used.
  • an additional step of drying the neutralized vegetable fat is performed after the second neutralization step and before the enzymatic transesterification step.
  • the process comprises an additional step of removing karitene.
  • the additional step of removing karitene is to be understood as removing karitene from a vegetable fat or fraction thereof in the method according to the invention.
  • This step of removing karitene may advantageously be performed after the soap residue removal step and before the fractionation step, or after the fractionation step and before the second neutralization step.
  • the karitene is preferably removed from the neutralized vegetable fat composition or from the first fraction.
  • the karitene may be removed by various suitable ways.
  • the invention furthermore relates to a system for processing a vegetable fat composition according to any of the above described embodiments, the system comprising a common processing line, a first processing line, and a first output, the common processing line comprising
  • processing line refers to a system, sub-system, and/or line of processing apparatuses or units, which together forms a processing line. These may preferably be connected directly as a continuous or un-broken processing line allowing the output of a given processing apparatus or unit to deliver its output to the next apparatus or unit, such as connection by piping allowing a liquid or partially liquid vegetable fat or oil to be moving by pumping.
  • a processing line may also be understood as being isolated apparatuses, units, or processing sub-lines, where the output of a given apparatus or unit is manually moved to the next apparatus, unit, or sub-line.
  • the above apparatuses or units may operate continuously, or batch-wise or as a combination thereof.
  • a processing line may preferably be located in the same facility, it is to be understood that it may extend over several facilities, with intermediate products being transported between such facilities.
  • a processing line may include one or more storage tanks for storage of intermediate products.
  • a processing line may be understood as a series of processing equipment adapted for performing processing of a vegetable fat composition according to an embodiment of the invention.
  • the separator unit is preferably a fractionation unit for performing a fractionation in accordance with any embodiment of the invention, i.e. preferably adapted to perform fractional crystallization.
  • said free fatty acid removal apparatus comprises
  • the free fatty acid removal apparatus comprises
  • said first output forms part of a second processing line, said second processing line comprising a mixing unit for mixing said second fraction with a palm oil mid fraction to obtain a second cocoa butter equivalent.
  • the valuable second cocoa butter equivalent may be obtained.
  • said first processing line furthermore comprises a mixing unit for mixing said transesterified first fraction with a palm oil mid fraction to obtain a first cocoa butter equivalent.
  • the valuable first cocoa butter equivalent may be obtained.
  • the invention relates to a method of processing shea fat and the process comprises the step of neutralizing the processed fat prior to a transesterification step.
  • the neutralization of the shea fat is performed subsequent to a soap residue removal step.
  • said neutralized first fraction is neutralized prior to said enzymatic transesterification step according to the method of any of the above embodiments.
  • a process for treatment of a vegetable fat composition VCF comprising a number of steps is provided.
  • the vegetable fat composition VCF is provided to the process.
  • the free fatty acids FFA are removed in a first neutralization step FNS, whereby a neutralized vegetable fat NVF is obtained.
  • the neutralized vegetable fat composition NVF is separated in a separation step FRA, preferably a fractionation, into a first fraction FF rich in StOO and/or OOO and a second fraction SF rich in StOSt.
  • a second base SB is added to the first fraction FF, thereby obtaining a neutralized first fraction NFF.
  • This neutralized first fraction NFF is fed into a reaction system comprising enzymes with transesterification activity to perform an enzymatic transesterification ETE, before finally obtaining a transesterified first fraction TFF from the reaction system.
  • the first neutralization step FNS of the above embodiment may according to another embodiment comprise a number of sub-steps, which are illustrated on figure 2 .
  • a base adding step BAS a first base FB is added to the vegetable fat composition VCF so as to saponify free fatty acids and obtaining a base added vegetable fat composition BAF.
  • the free fatty acids FFA are removed by separating the saponified free fatty acids SFA from the base added vegetable fat composition BAF, e.g. by centrifugation and/or washing followed by optional drying of the base added vegetable fat composition BAF.
  • a first acid FAC is added to the free fatty acid reduced vegetable fat FAR so as to convert or transform residues of saponified free fatty acids into free fatty acids.
  • a distillation step DIS is used as the first neutralization step FNS.
  • the vegetable fat composition VFC is distilled in the distillation step DIS so as to remove free fatty acids FFA and thereby obtaining a neutralized vegetable fat composition NVF.
  • This neutralized vegetable fat composition NVF is then processed according to the aforementioned embodiments.
  • a vegetable fat composition being shea fat 1 is provided.
  • the shea fat 1 may be refined and/or purified before being provided to the process of this embodiment.
  • an amount of a first base being a first sodium hydroxide aqueous solution 2 is added to the shea fat 1.
  • another base may be added, e.g. as an aqueous solution.
  • the first sodium hydroxide aqueous solution 2 reacts with free fatty acids in the shea fat 1 to saponify these free fatty acids, i.e. by transforming these free fatty acids into soaps. This reaction may be referred to as the base adding step 3.
  • This base adding step 3 increases the aqueous solubility of the free fatty acids in water.
  • the saponified free fatty acids or soaps 5 are then removed by a soap separation step 4.
  • This step 4 comprises centrifuging the shea fat 1 to separate the soap 5 and subsequent washing the shea fat 1 with water one or several times.
  • the shea fat 1 is dried, i.e. the water content of the shea fat 1 is lowered.
  • an amount of a first acid being an aqueous solution of citric acid 6 is added to the shea fat 1, so as to perform a conversion or transformation of the residual saponified free fatty acids in the shea oil 1, which were not removed by the centrifugation and washing 4, into free fatty acids.
  • the shea fat 1 is then subjected to a karitene removal step 8, where the karitene 10 can be removed. Then the shea fat 1, from which karitene 10 has been separated, is subjected to a fractionation 11 into a first fraction being an olein fraction 14, which is rich in StOO and/or OOO, and a second fraction being a stearin fraction 13, which is rich in StOSt.
  • a solvent 12 such as hexane
  • this fractionation 11 may be performed effectively. If the content of free fatty acids is too high, the crystallization properties of the shea fat 1, from which karitene has been separated, may be significantly altered, and the fractionation 11 becomes ineffective. Therefore, by removing the free fatty acids by the base adding step 3, the fractionation is made possible in relation to the crystallization properties. Furthermore, since the shea fat 1 is made soap free by the soap separation step 4 and the subsequent soap residue removal step 7 of adding citric acid 6, the fractionation 11 may be performed effectively without clogging of filters or other equipment used in the fractionation process 11.
  • the olein fraction 14 is then subjected to a second neutralization step 15, where a second base being a second sodium hydroxide aqueous solution 16 is added.
  • This second neutralization 15 lowers the concentration of acids, such as citric acid 6 or other acids, in the olein fraction 14.
  • the olein fraction 14 is subjected to a bleaching step 18 wherein an amount of bleaching earth 17 is added to the olein fraction 14.
  • the bleaching earth with impurities 19, such as saponified free fatty acids and other impurities, are subsequently removed by filtering 20.
  • the neutralized olein fraction 14 is then inputted into an enzymatic transesterification process 21, where it is put into contact with enzymes having transesterification activity and methyl stearate 22 added to the enzymatic transesterification step 21.
  • a transesterified shea olein 23 is obtained which has a significantly increased content of StOSt compared to the shea olein fraction 14 obtained from the fractionation 11.
  • a vegetable fat composition 1 is provided to the process.
  • a first base 2 is added to the vegetable fat composition 1, whereby a first neutralization 3 is obtained, transforming free fatty acids in the vegetable fat composition 1 into soaps 5, i.e. saponified free fatty acids.
  • soaps 5 are separated from the vegetable fat composition 1 by a soap separation step 4.
  • the soap separation step may e.g. comprise steps of centrifugation, washing with water, and drying.
  • residues of soap 5 may remain in the vegetable fat 1.
  • These residues of soap 5 are converted into free fatty acids by adding a first acid 6 to the vegetable fat 1.
  • the vegetable fat 1 is substantially free of soaps, and have only a small concentration of free fatty acids.
  • Such vegetable fats 1 are suitable for fractionation 11, and the vegetable fat 1 is therefore fractionated 11 into a stearin fraction 13 having a high melting point and an olein fraction 14 having a low melting point, i.e. the olein fraction 14 has a relatively low melting point relative to the stearin fraction 13.
  • the olein fraction 14 may be rich in StOO and/or OOO while the stearin fraction 13 may be rich in StOSt.
  • a second base 16 is added to the olein fraction 13 to facilitate a second neutralization 15, which neutralizes the first acid 6 and/or other acids in the olein fraction.
  • the olein fraction 13 is subjected to an enzymatic transesterification 18 by putting the olein fraction 13 into contact with enzymes having transesterification activity.
  • the enzymatic transesterification process 18 increases the relative content of StOSt, the longer the contact time between the vegetable oil and the enzymes, the higher the degree of conversion into StOSt may be realized in the transesterified vegetable oil 19.
  • the system comprises a common processing line CPL, a first processing line FPL, and a second processing line SPL.
  • the common processing line CPL comprises a free fatty acid removal apparatus FFR.
  • This free fatty acid removal apparatus may in one embodiment comprise a first base inlet FBI for adding said first base FB in said base adding step BAS, a soap separator SS for separating saponified free fatty acids SFA in said soap separation step SSS, and a first acid inlet FAI for adding said first acid FAC in said soap residue removal step SRR.
  • the common processing line CPL furthermore comprises a fractionation unit FU for performing the fractionation of said fractionation step FRA
  • the first processing line FPL which is adapted for said first fraction FF to be fed into, is connected to said fractionation unit FU.
  • the second processing line SPL which is adapted for said second fraction SF to be fed into, is connected to said fractionation unit FU.
  • the second processing line SPL comprises a second base inlet SBI for adding said second base SB in said second neutralization step SNS, and a reaction system RS for performing transesterification in said enzymatic transesterification step ETE.
  • the vegetable fat composition VFC is processed in a free fatty acid removal apparatus FFR in a common processing line CPL, where the free fatty acid removal apparatus FFR comprises a distillation unit DIU for distilling the vegetable fat composition VFC in the distillation step DIS to obtain separated free fatty acids FFA and a neutralized vegetable fat composition NVF.
  • the neutralized vegetable fat composition NVF may then be processed in processing equipment according to the aforementioned embodiments.
  • shea fat 20 kilograms (kg) of refined shea oil (shea fat) is provided.
  • One half of the shea oil (first half) is separated from the other half (second half) to give two chemically equivalent shea oil parts.
  • the second half of the shea oil from example 1 is subjected to the procedure according to example 2 similar to the first half, only leaving out the second neutralization step. Thereby a second shea olein portion is obtained.
  • the conversion efficiency of the first shea olein portion from example 3 and the second shea olein portion from example 2 is measured, by measuring the composition of methyl esters in the product by a GC (gas chromatography) method.
  • the amount of olein that has been processed by the transesterification enzymes, i.e. which has been converted, has been measured for the first shea olein portion in a first transesterification setup FSU, and for the second shea olein portion in a second transesterification setup SSU, where the second transesterification setup SSU is identical to the first transesterification setup FSU.
  • the normalized conversion-efficiency for the two setups is shown in figure 6 .
  • a half-value mass is determined, i.e. the amount of shea olein that can be processed before the conversion rate is reduced by half.
  • These half-value masses are 5398 and 3787 mass units of olein per mass unit of enzymes for the first setup FSU and second setup SSU, respectively. I.e. this experiment shows an increase of 43% in the half-value masses in the first setup FSU compared to the second setup SSU.
  • the absolute half-life of the enzymatic activity in the two setups FSU, SSU may change depending on the scaling, the ratio between the two half-value masses is concluded to be valid for industrial scale production.

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Claims (25)

  1. Procédé de traitement d'une composition de graisse végétale (VFC), le procédé comprenant les étapes consistant à
    - mettre à disposition la composition de graisse végétale (VFC),
    - dans une première étape de neutralisation (FNS), séparer les acides gras libres de la composition de graisse végétale (VFC) en obtenant ainsi une composition de graisse végétale neutralisée (NVF),
    - dans une étape de séparation (FRA), séparer la composition de graisse végétale neutralisée (NVF) en une première fraction (FF) riche en StOO et/ou OOO et en une seconde fraction (SF) riche en StOSt (où St = acide stéarique et O = acide oléique),
    - dans une seconde étape de neutralisation (SNS), ajouter à la première fraction (FF) une seconde base (SB) en obtenant ainsi une première fraction neutralisée (NFF),
    - introduire la première fraction neutralisée (NFF) et une source d'acide stéarique (SAS) dans une étape de transestérification enzymatique (ETE) qui permet de transestérifier la première fraction neutralisée (NFF) au moyen d'enzymes ayant une activité de transestérification 1,3-spécifique, en obtenant ainsi une première fraction transestérifiée (TFF).
  2. Procédé selon la revendication 1, dans lequel ladite première étape de neutralisation (FNS) comprend les étapes consistant à
    - dans une étape d'ajout de base (BAS), ajouter une première base (FB) à la composition de graisse végétale (VFC) en obtenant ainsi une composition de graisse végétale à base ajoutée (BAF),
    - dans une étape de séparation de savon (SSS), séparer les acides gras libres sous la forme d'acides gras libres saponifiés (SFA) de la composition de graisse végétale à base ajoutée (BAF) en obtenant ainsi une composition de graisse végétale réduite (FAR) ayant une teneur réduite en acides gras libres, et
    - dans une étape d'élimination de résidus de savon (SRR), ajouter un premier acide (FAC) à la composition de graisse végétale réduite (FAR) en obtenant ainsi la composition de graisse végétale neutralisée (NVF).
  3. Procédé selon la revendication 1, dans lequel ladite première étape de neutralisation (FNS) comprend une étape de distillation (DIS) consistant à distiller les acides gras libres (FFA) de la composition de graisse végétale (VFC) en obtenant ainsi une composition de graisse végétale neutralisée (NVF).
  4. Procédé selon la revendication 3, dans lequel ladite première étape de neutralisation (FNS) comprend en outre l'ajout d'un premier acide (FAC) à la composition de graisse végétale (VFC) avant l'étape de distillation (DIS).
  5. Procédé selon l'une quelconque des revendications 3 à 4, dans lequel ladite première étape de neutralisation (FNS) comprend en outre le blanchiment de ladite composition de graisse végétale (VFC) avant ladite étape de distillation (DIS).
  6. Procédé selon l'une quelconque des revendications précédentes, dans lequel la composition de graisse végétale (VFC) comprend de la graisse de karité.
  7. Procédé selon l'une quelconque des revendications précédentes, dans lequel la première fraction neutralisée (NFF) est blanchie.
  8. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'étape de séparation (FRA) implique une étape de fractionnement (FRA).
  9. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'étape de séparation de savon (SSS) comprend
    - la centrifugation de la composition de graisse végétale à base ajoutée (BAF) avec les acides gras libres saponifiés (SFA) de sorte à séparer les acides gras libres saponifiés (SFA) de la composition de graisse végétale à base ajoutée (BAF).
  10. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'étape de séparation de savon (SSS) comprend
    - le lavage de la composition de graisse végétale à base ajoutée (BAF).
  11. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'étape de séparation de savon (SSS) comprend
    - le séchage de la composition de graisse végétale à base ajoutée (BAF).
  12. Procédé selon l'une quelconque des revendications précédentes, dans lequel le premier acide (FAC) comprend de l'acide citrique.
  13. Procédé selon l'une quelconque des revendications précédentes, dans lequel le premier acide (FAC) transforme de quelconques acides gras libres saponifiés résiduels dans la composition de graisse végétale réduite (FAR) en acides gras libres.
  14. Procédé selon l'une quelconque des revendications précédentes, dans lequel les résidus d'acide citrique sont éliminés en ajoutant la seconde base (SB).
  15. Procédé selon l'une quelconque des revendications précédentes, dans lequel la première fraction neutralisée (NFF) est complètement neutralisée.
  16. Procédé selon l'une quelconque des revendications précédentes, dans lequel les enzymes ayant une activité de transestérification sont des enzymes 1,3-spécifiques.
  17. Procédé selon l'une quelconque des revendications précédentes, dans lequel une étape supplémentaire de séchage de la graisse végétale neutralisée (NFV) est réalisée après la seconde étape de neutralisation (SNS) et avant l'étape de transestérification enzymatique (ETE).
  18. Procédé selon l'une quelconque des revendications précédentes, où le procédé comprend une étape supplémentaire d'élimination de karitène.
  19. Système de traitement d'une composition de graisse végétale (VFC) selon l'une quelconque des revendications 1 à 18, le système comprenant une ligne de traitement commune (CPL), une première ligne de traitement (FPL), et une première sortie (FOP), la ligne de traitement commune (CPL) comprenant
    - un appareil d'élimination des acides gras libres (FFR), et
    - une unité de séparation (FU) pour réaliser la séparation de ladite étape de séparation (FRA),
    la première sortie (FOP) étant adaptée pour ladite première fraction (FF) devant être introduite dans, et étant connectée à, ladite unité de séparation (FU),
    la première ligne de traitement (FPL) étant adaptée pour ladite seconde fraction (SF) devant être introduite dans, et étant connectée à, ladite unité de séparation (FU), ladite première ligne de traitement (FPL) comprenant
    - une entrée pour une seconde base (SBI) afin d'ajouter ladite seconde base (SB) dans ladite seconde étape de neutralisation (SNS), et
    - un système de réaction (RS) pour réaliser la transestérification dans ladite étape de transestérification enzymatique (ETE).
  20. Système de traitement d'une composition de graisse végétale (VFC) selon la revendication 19, dans lequel l'appareil d'élimination des acides gras libres (FFR) comprend
    - une entrée pour une première base (FBI) afin d'ajouter ladite première base (FB) dans ladite étape d'ajout de base (BAS),
    - un séparateur de savon (SS) pour séparer les acides gras libres saponifiés (SFA) dans ladite étape de séparation de savon (SSS), et
    - une entrée pour un premier acide (FAI) afin d'ajouter ledit premier acide (FAC) dans ladite étape d'élimination de résidus de savon (SRR).
  21. Système de traitement d'une composition de graisse végétale (VFC) selon l'une quelconque des revendications 19 à 20, dans lequel ladite première sortie (FOP) fait partie d'une seconde ligne de traitement (SPL), ladite seconde ligne de traitement (SPL) comprenant
    - une unité de mélange pour mélanger ladite première fraction (FF) avec une fraction intermédiaire d'huile de palme afin d'obtenir un équivalent de beurre de cacao.
  22. Système de traitement d'une composition de graisse végétale (VFC) selon l'une quelconque des revendications 19 à 21, dans lequel ladite première ligne de traitement (FPL) comprend en outre une unité de mélange pour mélanger ladite première fraction transestérifiée (TFF) avec une fraction intermédiaire d'huile de palme afin d'obtenir un équivalent de beurre de cacao.
  23. Procédé de traitement de graisse de karité, où le procédé comprend l'étape consistant à neutraliser la graisse traitée avant une étape de transestérification.
  24. Procédé de traitement de graisse de karité selon la revendication 23, dans lequel la neutralisation de la graisse de karité est réalisée après une étape d'élimination de résidus de savon.
  25. Procédé de traitement de graisse de karité selon la revendication 23 ou 24, dans lequel ladite première fraction neutralisée (NFF) est neutralisée avant ladite étape de transestérification enzymatique (ETE) selon le procédé de l'une quelconque des revendications 1 à 18.
EP12772211.4A 2012-09-07 2012-09-07 Procédé de traitement d'une composition de graisse végétale Not-in-force EP2892986B1 (fr)

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CA1241227A (fr) 1981-07-08 1988-08-30 Alasdair R. Macrae Production de matiere grasse comestible
JP2722599B2 (ja) * 1989-02-03 1998-03-04 味の素株式会社 油脂の改質方法
EP1343860B1 (fr) 2000-12-21 2012-01-25 AarhusKarlshamn Denmark A/S Procede pour la preparation de fractions d'huile vegetale riches en matiere insaponifiable, non tocolique et a point de fusion eleve
ATE380877T1 (de) 2001-06-21 2007-12-15 T & T Oleochemie Gmbh Verfahren zur enzymatischen spaltung von ölen und fetten
CA2599499A1 (fr) 2005-02-28 2006-08-31 University Of Ottawa Appareil et procede pour la production de biocombustible
WO2009005767A1 (fr) 2007-06-29 2009-01-08 Archer-Daniels-Midland Company Procédé de dessalage de solutions de glycérol et de récupération des produits chimiques
JP5688207B2 (ja) 2009-03-03 2015-03-25 日清オイリオグループ株式会社 食用油の製造方法及び該方法により製造された食用油
EP2491128A1 (fr) 2009-10-21 2012-08-29 Novozymes A/S Procédé pour le traitement de l'huile
KR101314682B1 (ko) 2010-04-22 2013-10-07 씨제이제일제당 (주) 카카오 버터 유사 하드버터의 제조 방법
WO2011145101A1 (fr) 2010-05-18 2011-11-24 Premananda Das Huile d'argémone détoxifiée pour une utilisation comestible et non comestible

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DK2892986T3 (en) 2016-08-29
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JP2015534459A (ja) 2015-12-03
EP2892986A1 (fr) 2015-07-15
US20150291909A1 (en) 2015-10-15
JP6272869B2 (ja) 2018-01-31
WO2014037006A1 (fr) 2014-03-13
US9499768B2 (en) 2016-11-22

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